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Pyridine → HCID 86597333、化合物

HRID 2182192
ノート
印刷プレビュー

反応式

HRID 2182192 の反応式
[F:1][C:2]([F:16])([C:6]([F:15])([F:14])[C:7]([F:13])([F:12])[C:8]([F:11])([F:10])[F:9])[CH2:3][CH2:4][OH:5].N1C=CC=CC=1.[Cl-].[C:24]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41]CC)(=[O:30])/[CH:25]=[CH:26]\[C:27]([O-])=[O:28].C(OCC)(=O)C>C(Cl)(Cl)Cl>[C:24]([O:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])(=[O:30])/[CH:25]=[CH:26]\[C:27]([O:5][CH2:4][CH2:3][C:2]([F:16])([F:1])[C:6]([F:14])([F:15])[C:7]([F:12])([F:13])[C:8]([F:9])([F:10])[F:11])=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 748831-Hexanol, 3,3,4,4,5,5,6,6,6-nonafluoro-HCID 86759731HCID 86759731、化合物

生成物 1

HCID 86597333HCID 86597333、化合物収率 18%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

3,3,4,4,5,5,6,6,6-Nonafluorohexanol (164.6 g, 623 mmol) and pyridine (49.3 mL, 623 mmol) were dissolved in chloroform (280 mL), and the mixture was added dropwise with monododecyl maleate chloride (155.8 g, 566 mmol), while the internal temperature was kept at 20° C. or lower on an ice bath. After completion or the addition, the mixture was stirred for 1 hour and added with ethyl acetate. The organic phase was washed with 1 mol/L aqueous hydrochloric acid and a saturated sodium chloride aqueous solution. Then, the organic layer was collected, and the organic solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/chloroform=10/0 to 7/3 (v/v)) to obtain the target compound (48.2 g, yield: 18%).

後処理

  1. customwas kept at 20° C. or lower on an ice bath
  2. additionAfter completion or the addition
  3. washThe organic phase was washed with 1 mol/L aqueous hydrochloric acid
  4. customThen, the organic layer was collected
  5. customthe organic solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane/chloroform=10/0 to 7/3 (v/v))

出典と根拠

ORDレコード
ord-fa97ed03c95a4762b2eef0855df6058c
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06897013B2

反応ノート

読み込み中…

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